CN103121798A - Method for coating films with large area offline - Google Patents
Method for coating films with large area offline Download PDFInfo
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- CN103121798A CN103121798A CN2011103683764A CN201110368376A CN103121798A CN 103121798 A CN103121798 A CN 103121798A CN 2011103683764 A CN2011103683764 A CN 2011103683764A CN 201110368376 A CN201110368376 A CN 201110368376A CN 103121798 A CN103121798 A CN 103121798A
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Abstract
The invention relates to a method for coating films with large area offline. The method is characterized by including that a, precursor solution is gasified in a gasification device; b, the precursor gas obtained in the step a is carried by carrier gas to pass a pipeline to be delivered to a coating-film reactor; and c, the precursor gas sequentially passes a group of small gas cavities, being communicated with one another, of a gas feeding cavity to be mixed, and the evenly-mixed precursor gas is used for coating films on on-line glass in a coating-film chamber after passing a coating-film discharging port. By the aid of the proper precursor gas, one or two functional films with uniform thickness and no obvious optical interference fringes are evenly coated on the surface of moving large-size hot glass.
Description
Technical field
The present invention relates to a kind of offline large-area coating film method, it is to utilize aumospheric pressure cvd method (APCVD), deposit one or more oxide compound function films at mobile hot glass surface, these functional films comprise low radiation (Low-E) film, transparent conductive metal oxide compound (TCO) film, catalytic self-cleaning titanium deoxid film, intelligent thermochromism vanadium oxide film etc.
Background technology
Utilizing the aumospheric pressure cvd method is the method that realizes that at present glass functionization is the most frequently used at the sized rectangular glass substrate surface coating.The rete that this method makes is fine and close, is combined with matrix firmly, and deposition is good, thickness and more even, and film quality is more stable, is easy to realize producing in enormous quantities, and lot of domestic and international patent and document have related to the technique of this respect.
Chinese invention patent CN1145882A has set forth a kind of method of glass coating, deposition tin oxide base low radiation functions film on the mobile glass substrate of 630 ~ 640 ℃, but it does not relate to the description of structure of reactor; Chinese invention patent CN1792926A relates to a kind of apparatus for on-line coating film of float glass, utilizes this device can online production high quality and multi-functional coated glass, but this equipment is difficult to guarantee the homogeneity of rete; US Patent No. 20040175500A relates to the technique with the standby FTO nesa coating of aumospheric pressure cvd legal system, but does not relate to the description of structure of reactor.
Summary of the invention
The objective of the invention is to control the defective of difficulty in order to overcome the film thickness uniformity that exists in prior art, and a kind of offline large-area coating film method is provided.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of offline large-area coating film method is characterized in that:
A. in gasification installation, reaction precursor liquid is gasified;
B. then carried by pipeline by carrier gas and be delivered to the plated film reactor;
C. in the plated film reactor, precursor gas is carried out the precursor gas mixing through one group of little gas chamber that is connected of inlet chamber successively, and then even mixed precursor gas is through the online glass coating of plated film ejiction opening to coating chamber.
In the present invention, pipeline need to carry out omnidistance pipeline tracing and insulation, makes pipe temperature maintain a suitable temperature range, and the pipeline tracing mode comprises heat-conducting oil heating, electrically heated etc.
Plated film reactor in the present invention can effectively be controlled the homogeneity of air inlet, exhaust and the temperature of gas passage, thereby can guarantee fully that reactant gas reacts the homogeneity of film forming on whole substrate width, also reduces simultaneously the risk that pre-reaction and obstruction occur.
On the basis of above-mentioned main technical schemes, can increase following further perfect technical scheme:
Described inlet chamber is divided into two row 12 little gas chamber by the even gas distribution plate, even gas distribution plate between six little gas chamber on top is provided with one group of pore that arranges along the coating film production line width, even gas distribution plate between six little gas chamber of bottom has along the coating film production line width long strip shape narrow slit is set, precursor gas distributes through homogeneous phase after these 12 gas chamber, and then even mixed precursor gas process plated film ejiction opening is to online glass coating.
Described plated film reactor also has two discharge chambers, be provided with one group of round tube in each discharge chamber, having a narrow passage along the elongated direction setting of round tube between two adjacent round tubes is connected, a round tube of one end of the one group of round tube that is connected contacts bottom discharge chamber, the suction port that has one in the contact position links round tube and coating chamber, and a round tube of the other end is provided with the vapor pipe that links and communicates with the external world.
Described reaction precursor liquid can adopt precursor liquid for low radiation film, be used for the precursor liquid of transparent conductive metal sull, be used for the catalytic self-cleaning titanium deoxid film precursor liquid, be used for the precursor liquid of intelligent thermochromism vanadium oxide film.
Described carrier gas can be adopted nitrogen, helium.
The invention has the beneficial effects as follows and adopt the suitable gaseous state precursor can be at mobile hot one or more functional films of glass surface uniform deposition of large size, and film thickness be even, without obvious optical interference striped.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings:
Fig. 1 is front view of the present invention;
Fig. 2 is plated film reactor view of the present invention.
Embodiment
As shown in Figure 1, reaction precursor liquid is quantitatively gasification in gasification system 11, then carried by pipeline 12 by carrier gas and be delivered to plated film reactor 13, the plated film reactor of reactant gas process particular design is in mobile hot glass 14 surface reaction film forming, hot glass 14 type of drive are that live roll transmits, and transmission speed is electrodeless adjustable, and last waste gas is discharged by plated film reactor 13 exhaust-duct air inducing.
As shown in Figure 2, described plated film reactor, comprise an inlet chamber 1, two discharge chambers 2, four temperature control chambers 3 etc., reactant gas passes into inlet chamber 1 by inlet pipe 4 from the two ends of reactor, inlet chamber 1 is divided into 12 little gas chamber, along air flow line, distribution hole by the even gas distribution plate 6 that passes through particular design between the first six inlet chamber is connected, rear six air chamber are communicated by the narrow slit 7 of certain width, gas distributes through obtaining good homogeneous phase after the little inlet chamber of these 12 particular design, thereby can guarantee the homogeneity of reactor air inlet; Two discharge chambers 2 are symmetrical, internal structure is the same, respectively there is a vapor pipe 5 at discharge chamber 2 two ends, discharge chamber 2 is comprised of seven grades of circular passages that are similar to serpentine tube, connected by the narrow passage 10 of certain width between every grade of pipe, this pipe design can reduce resistance of exhaust on the one hand, prevents that passage from stopping up, and this serpentine design can guarantee the homogeneity of reactor exhaust on the other hand; Be provided with temperature control chamber 3 between the skin of discharge chamber and inlet chamber and discharge chamber, temperature control chamber 3 is interior can pass into according to the needs of actual production different circulatory mediators, intercepted the impact of plated film device outside temperature on the plated film gas temperature, to suppress the pre-reaction between gaseous feed.On each even gas distribution plate 6 of inlet chamber 1, the total area of distribution hole is corresponding with inlet chamber gas vent 8 areas, substantially is consistent, and narrow slit 7 width between rear six little gas chamber are identical with inlet chamber gas plated film mouth 8 width; In discharge chamber 2, narrow passage 10 sizes of connection pipes at different levels and the size of discharge chamber suction port 9 are consistent; The material of plated film reactor 13 can be any in graphite, fused quartz, corundum, stainless steel etc.
Specific embodiment 1
As shown in Figure 1, in the present embodiment, the temperature of glass substrate is 660 ℃, and glass substrate is the thick ultra-clear glasses of 4mm, and glass sheet size is 1200mm * 1000mm; Precursor liquid monobutyl-tin-trichloride (MBTC), trifluoroacetic acid (TFA), water (H2O) etc. quantitatively gasify in gasification system 11, then carried by pipeline by nitrogen and be delivered to plated film reactor 13, at last at mobile hot glass 14 surface deposition doped sno_2 fluorine nesa coatings (FTO).
After measured, the thickness of FTO transparency conducting layer is 680nm and even, the thickness deviation is ± 5% on the 1200mm plate width direction, the square resistance of rete is 7.9 Ω/, the electricalresistivityρ is 5.37 * 10-4 Ω/cm, the carrier concentration n of rete is 7.3 * 1020/cm3, and this transparent conductive film superior performance can be applicable to the devices such as thin-film solar cells fully.
As shown in Figure 1, in the present embodiment, the temperature of glass substrate is 620 ℃, and glass substrate is the 5mm simple glass, and glass sheet size is 1000mm * 1000mm; Precursor liquid vanadium tetrachloride (VCl4), tungsten hexachloride (WCl6), water (H2O) etc. quantitatively gasify in gasification system 11, then carried by pipe-line transportation system 12 by helium and be delivered to plated film reactor 13, at last at mobile hot glass 14 surface deposition low temperature intelligence thermochromism vanadium oxide films.After measured, the thickness of thermochromism vanadium oxide film is 120nm and even, and the thickness deviation is ± 5% on plate width direction, the thin film phase change invert point is 29 ℃, and visible light transmissivity is 43%, and this Low-temperature Thermochromic thin film phase change temperature is low, near room temperature, can be applicable to the intelligent devices such as smart window.
Claims (5)
1. offline large-area coating film method is characterized in that:
A. in gasification installation, reaction precursor liquid is gasified;
B. then carried by pipeline by carrier gas and be delivered to the plated film reactor;
C. in the plated film reactor, precursor gas is carried out the precursor gas mixing through one group of little gas chamber that is connected of inlet chamber successively, and then even mixed precursor gas is through the online glass coating of plated film ejiction opening to coating chamber.
2. a kind of offline large-area coating film method according to claim 1, it is characterized in that: described inlet chamber is divided into two row 12 little gas chamber by the even gas distribution plate, even gas distribution plate between six little gas chamber on top is provided with one group of pore that arranges along the coating film production line width, even gas distribution plate between six little gas chamber of bottom has along the coating film production line width long strip shape narrow slit is set, precursor gas distributes through homogeneous phase after this gas chamber of 12, and then even mixed precursor gas process plated film ejiction opening is to online glass coating.
3. a kind of offline large-area coating film method according to claim 2, it is characterized in that: described plated film reactor also has two discharge chambers, be provided with one group of round tube in each discharge chamber, having a narrow passage along the elongated direction setting of round tube between two adjacent round tubes is connected, a round tube of one end of the one group of round tube that is connected contacts bottom discharge chamber, the suction port that has one in the contact position links round tube and coating chamber, and a round tube of the other end is provided with the vapor pipe that links and communicates with the external world.
4. a kind of offline large-area coating film method according to claim 1 is characterized in that: described reaction precursor liquid can adopt precursor liquid for low radiation film, be used for the precursor liquid of transparent conductive metal sull, be used for the catalytic self-cleaning titanium deoxid film precursor liquid, be used for the precursor liquid of intelligent thermochromism vanadium oxide film.
5. a kind of offline large-area coating film method according to claim 1, it is characterized in that: described carrier gas can be adopted nitrogen, helium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110368376.4A CN103121798B (en) | 2011-11-19 | 2011-11-19 | A kind of offline large-area coating film method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110368376.4A CN103121798B (en) | 2011-11-19 | 2011-11-19 | A kind of offline large-area coating film method |
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| CN103121798A true CN103121798A (en) | 2013-05-29 |
| CN103121798B CN103121798B (en) | 2015-12-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113871539A (en) * | 2021-12-02 | 2021-12-31 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of perovskite solar cell |
| CN113948644A (en) * | 2021-10-15 | 2022-01-18 | 华能新能源股份有限公司 | CsPbBr3Preparation method of perovskite solar cell |
| CN116002988A (en) * | 2022-12-12 | 2023-04-25 | 玻璃新材料创新中心(安徽)有限公司 | Transparent conductive film glass for solar cell and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105180A (en) * | 1993-04-16 | 1995-07-12 | 利比-欧文斯-福特公司 | Method and apparatus for coating a glass substrate |
| CN1145882A (en) * | 1995-07-25 | 1997-03-26 | 皮尔金顿公共有限公司 | Method of coating glass |
| CN101892466A (en) * | 2010-06-25 | 2010-11-24 | 蚌埠玻璃工业设计研究院 | Offline large-area coating film production line |
-
2011
- 2011-11-19 CN CN201110368376.4A patent/CN103121798B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105180A (en) * | 1993-04-16 | 1995-07-12 | 利比-欧文斯-福特公司 | Method and apparatus for coating a glass substrate |
| CN1145882A (en) * | 1995-07-25 | 1997-03-26 | 皮尔金顿公共有限公司 | Method of coating glass |
| CN101892466A (en) * | 2010-06-25 | 2010-11-24 | 蚌埠玻璃工业设计研究院 | Offline large-area coating film production line |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113948644A (en) * | 2021-10-15 | 2022-01-18 | 华能新能源股份有限公司 | CsPbBr3Preparation method of perovskite solar cell |
| CN113871539A (en) * | 2021-12-02 | 2021-12-31 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of perovskite solar cell |
| CN113871539B (en) * | 2021-12-02 | 2022-03-01 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of perovskite solar cell |
| CN116002988A (en) * | 2022-12-12 | 2023-04-25 | 玻璃新材料创新中心(安徽)有限公司 | Transparent conductive film glass for solar cell and preparation method thereof |
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| CN103121798B (en) | 2015-12-16 |
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